CN114773941B - Super-amphiphobic nano coating liquid for PTFE (polytetrafluoroethylene) film - Google Patents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
- C09D133/16—Homopolymers or copolymers of esters containing halogen atoms
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
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Abstract
The invention provides a super-amphiphobic nano coating liquid for a PTFE film, and the preparation method comprises the following steps: mixing and stirring tetraethoxysilane, ethanol and water, adding ammonia water, and uniformly stirring to obtain a hydrophilic silicon dioxide solution; uniformly stirring a fluorine-containing acrylic ester monomer, acrylic acid and a solvent to form a mixed solution, dropwise adding an initiator into the mixed solution under the condition of introducing nitrogen, and heating until the reaction is finished to obtain a fluorine-containing hydrophilic polymer; the hydrophilic silica solution is mixed with the fluorine-containing hydrophilic polymer and then vigorously stirred to obtain the required coating liquid. The super-amphiphobic nano coating liquid for the PTFE membrane adopts nano particles and fluorine-containing polymer to form a core-shell structure, forms a nano particle layer on the surface of PTFE, and treats the PTFE membrane to obtain the super-amphiphobic coating, so that the super-amphiphobic coating is low in cost, environment-friendly, free of complex treatment steps and expensive instruments and equipment, has a large-scale industrial application prospect, and can create great economic benefits.
Description
Technical Field
The invention belongs to the field of hydrophobic and oleophobic coatings, and particularly relates to a super-amphiphobic nano coating liquid for a PTFE (polytetrafluoroethylene) film.
Background
At present, intelligent devices have become indispensable tools in life, such as intelligent household appliances including mobile phones, watches, headphones, intelligent sound boxes and the like. The acoustic and electrical components inside this device are very fragile and are subject to the intrusion of water, oil, solid particles (dust, waste, dangerous debris), resulting in damage to the device. The main solution is to add a protective layer at the position of the external through hole, and the protective layer is usually made of gauze, steel mesh or PTFE film material.
The hydrophobic and oleophobic properties of the surface of the material are improved in two directions: 1. the free energy of the surface of the material is reduced; 2. the surface roughness is improved. The lower the free energy of the material, the stronger the hydrophobicity; the microscopic roughness of the surface determines the hydrophilic and hydrophobic strength, with the coarser surface and the more hydrophobic. In recent years, theoretical researches on superhydrophobic surfaces have achieved a great deal of results, but methods for preparing superhydrophobic surfaces are not many, mainly include sol-gel methods, template methods, self-assembly methods, chemical etching methods and the like, and the methods have the problems of severe construction or use conditions, complicated steps, high cost and the like.
It is known to those skilled in the art that PTFE membranes themselves have a microporous structure to ensure breathability, and at the same time form a barrier at the through-hole location to effectively isolate dirt and dust. But PTFE membrane has weaker resistance to oil stains, and the phenomenon of infiltration of greasy dirt in life can occur, thereby affecting the permeability of sound and air and affecting the use effect. The special molecular structure of the PTFE molecules, which is hardly affected by any reagent because the C-C bond and the C-F bond cannot be contacted with the outside, endows the PTFE molecules with extremely good chemical stability, resists strong acid, strong alkali and corrosion of various chemical products, and simultaneously has extremely wide temperature resistance, and can be used for a long time within the temperature range of 180 ℃ below zero to 260 ℃, so that the PTFE is widely applied to the fields of aerospace, clothing, construction, electronics, chemical medical treatment and environmental protection filtration. However, due to the symmetrical molecular structure, the PTFE film has a nonpolar surface, is not easy to adsorb polar water, is easy to adhere polar oil, is easy to adsorb grease in the field of clothing fabrics, is difficult to maintain the cleanliness of the fabrics for a long time, and is also required to have a better hydrophobic and oleophobic effect because of the performance of the PTFE film, and particularly has extremely difficult improvement on oleophobic performance.
The fluorosilicone composite adhesive disclosed in the patent with publication No. CN10407116A has surface tension of 61 to water, propylene glycol, glycerol and the like, has an oleophobic angle of 150 degrees to substances close to water, and cannot have super-oleophobic effect to alkanes such as n-hexadecane and low-surface tension oil with the surface tension of about 27. The surface tension of most oils is around 30. Further, as mentioned in the patent publication No. CN112409916A and the patent publication No. CN103951279A, the super-lyophobic and lyophobic are aqueous emulsions, and the PTFE film cannot be wetted because of the strong water repellency of the PTFE film, so that the PTFE film cannot have super-oleophobic effect when being treated.
Disclosure of Invention
In view of the above, the present invention aims to provide a super-amphiphobic nano-coating solution for PTFE membrane, which has a good affinity with PTFE, and can directly treat the PTFE membrane to have super-amphiphobic performance.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a preparation method of super-amphiphobic nano-coating liquid for PTFE (polytetrafluoroethylene) films comprises the following steps:
s1: mixing and stirring tetraethoxysilane, ethanol and water, adding ammonia water, and uniformly stirring to obtain a hydrophilic silicon dioxide solution;
s2: uniformly stirring a fluorine-containing acrylic ester monomer, acrylic acid and a solvent to form a mixed solution, dropwise adding an initiator into the mixed solution under the condition of introducing nitrogen, and heating until the reaction is finished to obtain a fluorine-containing hydrophilic polymer;
s3: the hydrophilic silica solution is mixed with the fluorine-containing hydrophilic polymer and then vigorously stirred to obtain the required coating liquid.
The super-amphiphobic nano coating liquid for the PTFE membrane adopts the fluorine-containing polymer to embed nano particles to form a core-shell structure, and a nano particle layer is formed on the surface of PTFE through dipping treatment, so that the water contact angle and the oil contact angle of the super-amphiphobic material obtained through after-treatment reach 150 degrees, and the nano particles wrapped by the fluoride can obtain the super-amphiphobic nano material through a simple dipping process.
Further, in the step S1, the mass ratio of the tetraethoxysilane to the ethanol to the water to the ammonia water is 1:5-20:5-10:0.5-1, and the concentration of the ammonia water is 25%.
Further, in the step S2, the fluorine-containing acrylic ester monomer, the acrylic acid and the solvent are uniformly stirred to form a mixed solution, an initiator is dripped into the mixed solution at the constant temperature of 65 ℃ under the condition of introducing nitrogen, and the mixed solution is heated and kept at the temperature of 70 ℃ until the reaction is finished after the dripping is finished.
Further, the fluorine-containing acrylic ester monomer in the step S2 is a perfluorinated acrylic ester monomer; preferably, the fluorine-containing acrylate monomer is one or more of perfluoroalkyl ethyl acrylate, perfluorobutyl ethyl acrylate, perfluorohexyl ethyl acrylate and perfluorooctyl ethyl acrylate.
Further, in the step S2, the solvent is a mixed solution of tetrahydrofuran and perfluoro-cyclic ether.
Further, the mass ratio of the fluorine-containing acrylate monomer to the acrylic acid in the step S2 is 6-9.5:0.5-4.
Further, the initiator in the step S2 is azodiisobutyronitrile, and the addition amount of the initiator is 0.5-5% of the mass of the mixed solution.
Further, the mass of the hydrophilic silica solution in the step S3 is 1% -20% of the mass of the fluorine-containing hydrophilic polymer.
Further, the method comprises the following steps:
s1: mixing and stirring tetraethoxysilane, ethanol and water, adding ammonia water, and uniformly stirring to obtain a hydrophilic silicon dioxide solution, wherein the mass ratio of the tetraethoxysilane to the ethanol to the water to the ammonia water is 1:17:6:0.7, and the concentration of the ammonia water is 25%;
s2: uniformly stirring a fluorine-containing acrylate monomer, acrylic acid and a solvent to form a mixed solution, wherein the mass ratio of the fluorine-containing acrylate monomer to the acrylic acid is 8:2, the solvent is a mixed solution of tetrahydrofuran and perfluorinated cyclic ether, the dosage ratio of the tetrahydrofuran to the perfluorinated cyclic ether is 1:5, dropwise adding azodiisobutyronitrile into the mixed solution at the constant temperature of 65 ℃ under the condition of introducing nitrogen, adding azodiisobutyronitrile with the addition amount of 1% of the mass of the mixed solution, heating and preserving the heat at 70 ℃ until the reaction is finished after the dropwise adding is finished, and obtaining a fluorine-containing hydrophilic polymer;
s3: and (3) mixing the hydrophilic silicon dioxide solution with the fluorine-containing hydrophilic polymer, and then stirring vigorously to obtain the required coating liquid, wherein the mass of the hydrophilic silicon dioxide solution is 5% of that of the fluorine-containing hydrophilic polymer.
The super-amphiphobic nano coating liquid for the PTFE membrane, which is obtained by the preparation method, has the advantages of simple use method, and can be directly obtained by diluting and dispersing the super-amphiphobic nano coating liquid into 0.5% solution by using fluorine-containing cyclic ether and coating the solution on a substrate by an impregnation process.
Compared with the prior art, the super-amphiphobic nano-coating liquid for the PTFE membrane has the following advantages:
the super-amphiphobic nano coating liquid for the PTFE membrane adopts nano particles and fluorine-containing polymer to form a core-shell structure, a nano particle layer is formed on the surface of PTFE, the PTFE membrane is treated, the water contact angle and the oil contact angle of the obtained super-amphiphobic coating reach 150 degrees, the coating can be directly formed by coating the base material through an impregnation process, the cost is low, the environment is protected, no complex treatment step is needed, expensive instruments and equipment are not needed, the super-amphiphobic nano coating liquid is suitable for preparing a large amount of super-hydrophobic coating liquid on the surface of the relevant base material, the application prospect of large-scale industrialization is realized, and great economic benefits can be created.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
1g of tetraethyl orthosilicate (TEOS), 5g of ethanol and 5g of water are mixed and stirred for 10-20 minutes, then 0.5 ammonia water is added, and the mixture is stirred at constant temperature for 2 hours to prepare a hydrophilic silica solution for standby. 8g of fluorine-containing acrylic ester monomer and 2g of acrylic acid are taken and added into a three-mouth bottle, 10g of tetrahydrofuran and 1g of perfluoro-cyclic ether are added, the stirring is uniform, under the condition of introducing nitrogen, azodiisobutyronitrile is slowly added dropwise at the constant temperature of 65 ℃, after the dropwise addition is finished, the temperature is raised to 70 ℃ for reaction for 6 hours, 1g of standby hydrophilic silicon dioxide solution is poured into fluorine-containing hydrophilic polymer, the stirring is violent, and simultaneously 90g of perfluoro-cyclic ether is added, so that the super-amphiphobic nano coating liquid is prepared.
Example 2
1g of tetraethyl orthosilicate (TEOS), 17g of ethanol and 6g of water are mixed and stirred for 10-20 minutes, then 0.7 ammonia water is added, and the mixture is stirred at constant temperature for 2 hours to prepare a hydrophilic silica solution for standby. 8g of fluorine-containing acrylic ester monomer and 2g of acrylic acid are taken and added into a three-mouth bottle, 10g of tetrahydrofuran and 1g of perfluoro-cyclic ether are added, the stirring is uniform, under the condition of introducing nitrogen, azodiisobutyronitrile is slowly added dropwise at the constant temperature of 65 ℃, after the dropwise addition is finished, the temperature is raised to 70 ℃ for reaction for 6 hours, 1g of standby hydrophilic silicon dioxide solution is poured into fluorine-containing hydrophilic polymer, the stirring is violent, and simultaneously 90g of perfluoro-cyclic ether is added, so that the super-amphiphobic nano coating liquid is prepared.
Example 3
1g of tetraethyl orthosilicate (TEOS), 17g of ethanol and 6g of water are mixed and stirred for 10-20 minutes, then 0.7 ammonia water is added, and the mixture is stirred at constant temperature for 2 hours to prepare a hydrophilic silica solution for standby. 8g of fluorine-containing acrylic ester monomer and 2g of acrylic acid are taken and added into a three-mouth bottle, 10g of tetrahydrofuran and 1g of perfluorinated cyclic ether are added, the stirring is uniform, under the condition of introducing nitrogen, azodiisobutyronitrile is slowly added dropwise at the constant temperature of 65 ℃, after the dropwise addition is finished, the temperature is raised to 70 ℃ for reaction for 6 hours, 0.5g of standby hydrophilic silicon dioxide solution is poured into fluorine-containing hydrophilic polymer, the stirring is vigorously carried out, and simultaneously 90g of perfluorinated cyclic ether is added, so that the super-amphiphobic nano coating liquid is prepared.
Example 4
1g of tetraethyl orthosilicate (TEOS), 17g of ethanol and 6g of water are mixed and stirred for 10-20 minutes, then 0.7 ammonia water is added, and the mixture is stirred at constant temperature for 2 hours to prepare a hydrophilic silica solution for standby. 7g of fluorine-containing acrylic ester monomer and 3g of acrylic acid are taken and added into a three-mouth bottle, 10g of tetrahydrofuran and 1g of perfluorinated cyclic ether are added, the stirring is uniform, under the condition of introducing nitrogen, azodiisobutyronitrile is slowly added dropwise at the constant temperature of 65 ℃, after the dropwise addition is finished, the temperature is raised to 70 ℃ for reaction for 6 hours, 0.5g of standby hydrophilic silicon dioxide solution is poured into fluorine-containing hydrophilic polymer, the stirring is vigorously carried out, and simultaneously 90g of perfluorinated cyclic ether is added, so that the super-amphiphobic nano coating liquid is prepared.
Comparative example 1
The difference from example 1 is that the amounts of ethyl orthosilicate, ethanol and water used in step S1 of comparative example 1 were 1g, 10g and 16g, respectively, and the other steps were the same as in example 1.
Comparative example 2
The difference from example 1 is that no ammonia was added in step S1 of comparative example 2.
Comparative example 3
The difference from example 1 is that the solvent in step S2 of comparative example 3 is ethyl acetate.
The emulsion prepared in the above examples was subjected to a hydrophobic oleophobic test by the following method: the emulsion obtained above was diluted and dispersed with a perfluoro cyclic ether to a 0.5% solution, which was coated on a PTFE film by an immersion process to test the contact angle of water and oil (HD).
Table 1-4 test results
The invention adopts the fluorine-containing polymer to embed the nano particles to form a core-shell structure, and the core-shell structure and the fluorine-containing polymer have the synergistic effect. Besides providing hydrophobic and oleophobic properties, the nano silicon dioxide can also improve the problems of poor suspension stability, poor weather resistance, poor washing resistance and the like of the nano liquid, so that the bonding strength of a coating film and PTFE is greatly improved, the hardness of the coating film is increased, and the self-cleaning capability of the surface is also improved; the perfluorinated hydrophilic polymer plays a role in hydrophobic and oleophobic to a certain extent, the super-hydrophobic and super-oleophobic performance is further improved by compounding and using the perfluorinated hydrophilic polymer, and molecules of the solvent perfluorinated cyclic ether can permeate into the substrate, so that deep long-term hydrophobic and antifouling protection is achieved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (3)
1. The preparation method of the super-amphiphobic nano coating liquid for the PTFE membrane is characterized by comprising the following steps of:
s1: mixing and stirring tetraethoxysilane, ethanol and water, adding ammonia water, and uniformly stirring to obtain a hydrophilic silicon dioxide solution;
s2: uniformly stirring a fluorine-containing acrylic ester monomer, acrylic acid and a solvent to form a mixed solution, dropwise adding an initiator into the mixed solution at the constant temperature of 65 ℃ under the condition of introducing nitrogen, heating and preserving the temperature of 70 ℃ until the reaction is finished after the dropwise adding is finished to obtain a fluorine-containing hydrophilic polymer, wherein the mass ratio of the fluorine-containing acrylic ester monomer to the acrylic acid is 6-9.5:0.5-4, the solvent is the mixed solution of tetrahydrofuran and perfluoro cyclic ether, the fluorine-containing acrylic ester monomer is one or more of perfluoroalkyl ethyl acrylate, perfluorobutyl ethyl acrylate, perfluorohexyl ethyl acrylate and perfluorooctyl ethyl acrylate, the initiator is azodiisobutyronitrile, and the adding amount of the initiator is 0.5-5% of the mass of the mixed solution;
s3: and (3) mixing the hydrophilic silicon dioxide solution with the fluorine-containing hydrophilic polymer, and then stirring vigorously to obtain the required coating liquid, wherein the mass of the hydrophilic silicon dioxide solution is 1-20% of that of the fluorine-containing hydrophilic polymer.
2. The method for preparing the super-amphiphobic nano-coating liquid for PTFE films according to claim 1, characterized by: in the step S1, the mass ratio of the tetraethoxysilane to the ethanol to the water to the ammonia water is 1:5-20:5-10:0.5-1, and the concentration of the ammonia water is 25%.
3. A super-amphiphobic nano-coating liquid for PTFE membranes obtained according to the preparation method of claim 1 or 2.
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